TW201823394A - Chemical mechanical polishing composition and chemical mechanical polishing method capable of realizing good polishing characteristics while suppressing corrosion of cobalt film - Google Patents
Chemical mechanical polishing composition and chemical mechanical polishing method capable of realizing good polishing characteristics while suppressing corrosion of cobalt film Download PDFInfo
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[0001] 本發明為關於一種化學機械研磨用組成物以及使用其之化學機械研磨方法。[0001] The present invention relates to a chemical mechanical polishing composition and a chemical mechanical polishing method using the same.
[0002] 伴隨著半導體裝置之高精細化，形成於半導體裝置內之配線以及插頭等而成之配線層的微細化逐漸進步。伴隨於此，有使用以化學機械研磨（以下亦稱作「CMP」）將配線層變得更平坦化之方法。近年來，微細化為10nm節點以上時，要求於此等之導電體金屬適用鈷，並將剩餘所積層之鈷以CMP有效率地去除，且同時抑制反應性較高之鈷的腐蝕，能夠形成良好的表面狀態。 [0003] 關於如此之鈷層以及鈷插頭（以下亦稱作「鈷膜」）之化學機械研磨，例如專利文獻1中有揭示一種pH5以上8.3以下之中性區域之化學機械研磨用組成物，其係作為相當於第1研磨處理步驟之完成研磨之前階段所使用之半導體研磨用組成物，且包含胺基酸、含氮之雜環化合物、研磨粒。 [0004] 且，專利文獻2中有揭示一種化學機械研磨方法，其係包含氧化劑等之鈷之蝕刻劑、鈷研磨速度提升劑、腐蝕阻礙劑，且使用pH7以上12以下之鹼區域之化學機械研磨用組成物來研磨包含鈷之基材。此研磨方法中所使用之化學機械研磨用組成物有揭示由塔菲爾圖（Tafel plot）所定量之鈷之腐蝕電位為0mV以上正電位。 [0005] 進而，專利文獻3中有揭示一種化學機械研磨方法，其係包含氧化劑等之鈷之蝕刻劑、金屬防蝕劑以及水，且使用pH4以下之酸性區域之化學機械研磨用組成物來研磨包含鈷之基材。 [先前技術文獻] [專利文獻] [0006] [專利文獻1] 日本特開2016-30831號公報 [專利文獻2] 日本特開2016-58730號公報 [專利文獻3] 國際公開第2016/98817號[0002] With the high definition of semiconductor devices, the miniaturization of wiring layers formed by wirings, plugs, and the like formed in semiconductor devices has gradually progressed. Along with this, there is a method of flattening the wiring layer by chemical mechanical polishing (hereinafter also referred to as "CMP"). In recent years, when the micronization is more than 10nm node, it is required to apply cobalt to these conductive metals, and effectively remove the remaining layer of cobalt by CMP, and at the same time suppress the corrosion of the highly reactive cobalt to form Good surface condition. [0003] Regarding the chemical mechanical polishing of such a cobalt layer and a cobalt plug (hereinafter also referred to as “cobalt film”), for example, Patent Document 1 discloses a chemical mechanical polishing composition for a neutral region having a pH of 5 to 8.3. It is a composition for semiconductor polishing which is equivalent to the first polishing process step before the polishing is completed, and contains an amino acid, a nitrogen-containing heterocyclic compound, and polishing particles. [0004] In addition, Patent Document 2 discloses a chemical-mechanical polishing method that uses an etchant containing cobalt, such as an oxidizing agent, a cobalt polishing rate enhancer, and a corrosion inhibitor, and uses a chemical machine in an alkaline region having a pH of 7 to 12 The polishing composition is used to polish a substrate containing cobalt. The chemical mechanical polishing composition used in this polishing method has revealed that the corrosion potential of cobalt as quantified by a Tafel plot is a positive potential of 0 mV or more. [0005] Furthermore, Patent Document 3 discloses a chemical mechanical polishing method which uses an etchant of cobalt such as an oxidizing agent, a metal anticorrosive, and water, and uses a chemical mechanical polishing composition in an acidic region having a pH of 4 or less for polishing. Substrate containing cobalt. [Prior Art Literature] [Patent Literature] [0006] [Patent Literature 1] Japanese Patent Laid-Open No. 2016-30831 [Patent Literature 2] Japanese Patent Laid-Open No. 2016-58730 [Patent Literature 3] International Publication No. 2016/98817
[本發明欲解決之課題] [0007] 然而，使用以往之酸性金屬膜研磨用之化學機械研磨用組成物，以化學機械研磨來研磨如鈷之金屬膜時，鈷膜會容易溶解，會招致鈷配線之異常氧化或腐蝕、斷線、消失之問題。且，以往之鹼性金屬研磨用之化學機械研磨用組成物，鈷膜在化學性上較安定，且硬度較高，故有不容易有效率地來研磨之問題。 [0008] 於此，本發明相關之幾個型態為提供一種半導體裝置之製造有用之化學機械研磨用組成物以及使用其之化學機械研磨方法，其係能夠解決上述課題中至少一部分，且抑制鈷膜之腐蝕，並同時實現良好之研磨特性。 [解決課題之手段] [0009] 本發明為用來解決上述課題中至少一部分者，能夠作為以下型態或適用例來實現。 [0010] [適用例1] 本發明相關之化學機械研磨用組成物之一型態，其特徵為含有氫硫基介由共價鍵而被固定化於表面之研磨粒與液狀介質。 [0011] [適用例2] 適用例1之化學機械研磨用組成物中， 進一步含有鉀以及鈉， 將前述鉀之含量設為MK （ppm），且將前述鈉之含量設為MNa （ppm）時，MK /MNa =3×103 ~3×105 。 [0012] [適用例3] 適用例1或適用例2之化學機械研磨用組成物中， 前述研磨粒之長徑（Rmax）與短徑（Rmin）之比（Rmax/Rmin）能夠為1.0以上1.5以下。 [0013] [適用例4] 適用例1至適用例3中任一例之化學機械研磨用組成物中， pH能夠為7以上11以下。 [0014] [適用例5] 適用例1至適用例4中任一例之化學機械研磨用組成物中， 進一步含有具有一個以上雙鍵之陰離子性化合物， 前述具有一個以上雙鍵之陰離子性化合物之含量能夠為0.001質量%以上1質量%以下。 [0015] [適用例6] 適用例1至適用例5中任一例之化學機械研磨用組成物能夠使用在將鈷膜進行化學機械研磨之用途。 [0016] [適用例7] 本發明相關之化學機械研磨方法之一型態，其特徵為包含使用適用例1至適用例6中任一例之化學機械研磨用組成物，將鈷膜進行化學機械研磨之步驟。 [發明效果] [0017] 藉由本發明相關之化學機械研磨用組成物，在半導體裝置之製造中，能夠抑制鈷膜之腐蝕，同時實現良好之研磨特性。因此，本發明相關之化學機械研磨用組成物，在將作為配線材料之鈷膜作為研磨對象之CMP特別有用。[Problems to be Solved by the Invention] [0007] However, when a chemical mechanical polishing composition for polishing an acidic metal film in the past is used to polish a metal film such as cobalt by chemical mechanical polishing, the cobalt film is easily dissolved, which may cause dissolution. Cobalt wiring is subject to abnormal oxidation or corrosion, disconnection, and disappearance. In addition, the conventional chemical mechanical polishing composition for alkaline metal polishing has a problem in that the cobalt film is chemically stable and has a high hardness, so that it is not easy to efficiently polish. [0008] Herein, several aspects related to the present invention are to provide a chemical mechanical polishing composition useful for the manufacture of semiconductor devices and a chemical mechanical polishing method using the same, which can solve at least a part of the above problems and suppress Corrosion of the cobalt film, while achieving good abrasive properties. [Means for Solving the Problem] [0009] The present invention is to solve at least a part of the problems described above, and can be implemented as the following forms or application examples. [Application Example 1] A type of the chemical mechanical polishing composition according to the present invention is characterized in that it contains abrasive particles and a liquid medium that are fixed on the surface through a covalent bond through a hydrogen-sulfur group. [0011] Application Example 2 The chemical mechanical polishing composition of Application Example 1 further contains potassium and sodium, and the content of the potassium is set to M K (ppm), and the content of the sodium is set to M Na ( ppm), M K / M Na = 3 × 10 3 to 3 × 10 5 . [0012] [Application Example 3] In the chemical mechanical polishing composition of Application Example 1 or Application Example 2, the ratio (Rmax / Rmin) of the long diameter (Rmax) to the short diameter (Rmin) of the abrasive grains can be 1.0 or more. 1.5 or less. [0013] [Application Example 4] In the chemical mechanical polishing composition of any of Application Examples 1 to 3, the pH can be 7 or more and 11 or less. [Application Example 5] The chemical mechanical polishing composition of any of Application Examples 1 to 4 further contains an anionic compound having one or more double bonds, and the aforementioned anionic compound having one or more double bonds. The content can be 0.001% by mass or more and 1% by mass or less. [Application Example 6] The chemical mechanical polishing composition of any one of Application Examples 1 to 5 can be used for a chemical mechanical polishing of a cobalt film. [Applicable Example 7] One form of a chemical mechanical polishing method related to the present invention is characterized by including using a chemical mechanical polishing composition of any one of Application Examples 1 to 6 to chemically mechanically coat a cobalt film. Steps of grinding. [Inventive Effect] [0017] With the chemical mechanical polishing composition according to the present invention, in the manufacture of a semiconductor device, it is possible to suppress corrosion of a cobalt film and achieve good polishing characteristics. Therefore, the chemical mechanical polishing composition according to the present invention is particularly useful in CMP in which a cobalt film as a wiring material is polished.
[實施發明之形態] [0019]以下，針對本發明之適合的實施形態進行詳細地說明。且，本發明不限定於下述之實施形態，在不變更本發明之要旨的範圍內，亦可包含實施之各種變形例。 [0020] 1.化學機械研磨用組成物 本發明之一實施形態相關之化學機械研磨用組成物之特徵為含有氫硫基介由共價鍵而被固定化於表面之研磨粒與液狀介質。以下，針對本實施形態相關之化學機械研磨用組成物進行詳細地說明。 [0021] 1.1.研磨粒 本實施形態相關之化學機械研磨用組成物含有氫硫基（-SH）介由共價鍵合而被固定化於表面之研磨粒。本實施形態中所使用之研磨粒由於為氫硫基介由共價鍵固定於其表面之研磨粒，故並不包含如其表面上具有氫硫基之化合物為物理性或離子性吸著之研磨粒。 [0022] 本實施形態中所使用之研磨粒之材質並無特別限制，有舉出二氧化矽、二氧化鈰、氧化鋁、二氧化鋯、氧化鈦等，但為二氧化矽較佳。氫硫基（-SH）介由共價鍵而被固定化於表面之二氧化矽粒子能夠由例如以下來製造。 [0023] 首先，準備二氧化矽粒子。作為二氧化矽粒子，有舉例如煅製二氧化矽、膠體二氧化矽等，但以降低刮痕等之研磨缺陷之觀點來看，為膠體二氧化矽較佳。作為膠體二氧化矽，能夠使用以例如特開2003-109921號公報等中記載之方法所製造者。 [0024] 二氧化矽粒子之表面修飾能夠適用日本特開2010-269985號公報或J.Ind.Eng.Chem., Vol.12,No.6,(2006) 911-917等中記載之方法。具體來說，能夠藉由如下來製造，將二氧化矽粒子與含氫硫基之矽氧烷耦合劑於酸性介質中充分地攪拌，使含氫硫基之矽氧烷耦合劑共價鍵於該二氧化矽粒子之表面。作為含氫硫基之矽氧烷耦合劑，有舉例如3-硫氫基丙基甲基二甲氧基矽氧烷、3-硫氫基丙基三甲氧基矽氧烷等。 [0025] 如此所得之二氧化矽粒子為氫硫基介由共價鍵而被固定於表面。因此，化學機械研磨用組成物中，二氧化矽粒子之表面會藉由該官能基而負向地充電，二氧化矽粒子變得容易吸著於鈷膜之表面。其結果，由於二氧化矽粒子會在鈷膜之表面局部化，因此，機械性的研磨力會提高，對鈷膜之研磨速度也會提升。 [0026] 研磨粒之表面電位（Zeta電位）在化學機械研磨用組成物之pH為7以上11以下之區域中為負電位，其負電位為-20mV以下較佳。Zeta電位為-20mV以下的話，則如上述，研磨粒會容易吸著於鈷膜之表面，故對鈷膜之研磨速度會提升。作為Zeta電位測定裝置，有舉出大塚電子股份公司製之「ELSZ-1」、Malvern公司製之「Zetasizer nanozs」等。研磨粒之Zeta電位能夠以增減上述含氫硫基之矽氧烷耦合劑的添加量來適當地調整。 [0027] 研磨粒之平均粒子徑能夠藉由以動力光散射法作為測定原理之粒度分布測定裝置來測定後求出。研磨粒之平均粒子徑較佳為15nm以上100nm以下，再較佳為20nm以上80nm以下，特別佳為30nm以上70nm以下。研磨粒之平均粒子徑若在前述範圍，則能夠得到達成對鈷膜之實用上的研磨速度，同時難以產生研磨粒之沉降･分離且儲藏安定性優異之化學機械研磨用組成物。作為以動力光散射法作為測定原理之粒度分布測定裝置，有舉出Beckman･Coulter公司製之奈米粒子分析儀「DelsaNano S」；Malvern公司製之「Zetasizer nano zs」；股份公司堀場製作所製之「LB550」等。且，使用動力光散射法所測定之平均粒子徑表示複數個一次粒子凝集所形成之二次粒子之平均粒子徑。 [0028] 研磨粒之長徑（Rmax）與短徑（Rmin）之比Rmax/Rmin較佳為1.0~1.5、再較佳為1.0~1.4，特別佳為1.0~1.3。Rmax/Rmin若在前述範圍內，則不會引起研磨對象之鈷膜的缺陷，能夠使高研磨速度與高平坦化特性兩立。 [0029] 於此，研磨粒之長徑（Rmax）意指關於以透過型電子顯微鏡所攝影的一個獨立之研磨粒的影像，連接影像之端部與端部之直線中最長之直線的距離。研磨粒之短徑（Rmin）意指關於以透過型電子顯微鏡所攝影的一個獨立之研磨粒的影像，連接像之端部與端部之直線中最短之直線的距離。 [0030] 例如，如圖1所示，以透過型電子顯微鏡所攝影的一個獨立之研磨粒10a的影像為橢圓形狀時，將其橢圓形狀之長軸a判斷為研磨粒之長徑（Rmax），將短軸b判斷為研磨粒之短徑（Rmin）。如圖2所示，以透過型電子顯微鏡所攝影之一個獨立之研磨粒10b的影像為2個一次粒子之凝集體時，將連接影像之端部與端部之直線中最長之距離c判斷為研磨粒之長徑（Rmax），將連接影像之端部與端部之直線中最短徑d判斷為研磨粒之短徑（Rmin）。如圖3所示，以透過型電子顯微鏡所攝影之一個獨立之研磨粒10c的影像為3個以上之一次粒子之凝集體時，將連接影像之端部與端部之直線中最長距離e判斷為研磨粒之長徑（Rmax），將連接影像之端部與端部之直線中最短徑f判斷為研磨粒之短徑（Rmin）。 [0031] 藉由如上述之判斷手法，能夠例如測定50個研磨粒之長徑（Rmax）與短徑（Rmin），算出長徑（Rmax）以及短徑（Rmin）之平均值後，再藉由計算其長徑之平均值與短徑之平均值之比（Rmax/Rmin）來求出。 [0032] 研磨粒之含量相對於化學機械研磨用組成物之全質量，較佳為1~20質量%，再較佳為1~15質量%，特別佳為1~10質量%。研磨粒之含有比例若在前述範圍，則會得到對鈷膜之充分的研磨速度，且化學機械研磨用組成物中之研磨粒之分散安定性良好。 [0033] 1.2.液狀介質 本實施形態相關之化學機械研磨用組成物含有液狀介質。作為液狀介質，有舉出水、水以及乙醇之混合介質、包含水以及具有與水之相溶性之有機溶媒之混合介質等。此等之中，使用水、水以及乙醇之混合介質較佳，使用水再較佳。 [0034] 1.3.其他成分 本實施形態相關之化學機械研磨用組成物除了上述成分以外，能夠含有具有一個以上雙鍵之陰離子性化合物、鉀以及鈉、防蝕劑、特開2014-229827號公報等中記載之公知的有機酸（惟，除了具有一個以上雙鍵之陰離子性化合物之外）、界面活性劑等之添加劑。 [0035] ＜具有一個以上雙鍵之陰離子性化合物＞ 本實施形態相關之化學機械研磨用組成物含有具有一個以上雙鍵之陰離子性化合物較佳。如此之陰離子性化合物在經改質之鈷膜表面中，能夠與鈷原子形成螯合。藉此，化學機械研磨用組成物中會溶出鈷，有時鈷膜之研磨速度會提升。 [0036]作為具有一個以上雙鍵之陰離子性化合物，為下述一般式（1）~（3）所表示之化合物再較佳。 [0037]（上述一般式（1）中，R1 為碳數1~8之烷基或羧基，R2 表示具有羧基之碳數1~15之有機基或羧基。） [0038][0039][0040] 上述一般式（2）以及上述一般式（3）中，R3 、R4 、R5 以及R6 各自獨立表示氫或具有羧基之碳數1~3之有機基或羧基。惟，R3 以及R4 之至少一者表示具有羧基之碳數1~3之有機基或羧基，R5 以及R6 之至少一者表示具有羧基之碳數1~3之有機基或羧基。 [0041] 作為具有一個以上雙鍵之陰離子性化合物之具體例，有舉例如馬來酸、丁烯二酸、喹啉酸、喹哪啶酸、油酸、烯基琥珀酸以及此等之鹽等，能夠使用此等之1種以上。 [0042] 具有一個以上雙鍵之陰離子性化合物之含量相對於化學機械研磨用組成物之全質量，較佳為0.0001~1質量%，再較佳為0.001~0.5質量%。具有一個以上雙鍵之陰離子性化合物之含有比例若在前述範圍，則能抑制鈷膜之腐蝕，同時對鈷膜之研磨速度會提升。 [0043] ＜鉀以及鈉＞ 本實施形態相關之化學機械研磨用組成物含有鉀以及鈉較佳。一般來說，如日本特開2000-208451號公報等中記載，於半導體之製造步驟中，鈉或鉀等鹼金屬被認為是一種應盡可能去除之雜質。因此，化學機械研磨用組成物等之半導體處理中所使用之各種組成物中，作為用來控制pH之鹼基，並非氫氧化鈉等之無機鹼基，使用氫氧化四甲基銨（TMAH）等之有機鹼基較佳。然而，本案發明中，研磨步驟中，藉由使用以特定比例含有鉀以及鈉之化學機械研磨用組成物，不會使半導體特性大幅地惡化，反而具有使處理特性提升之效果。 [0044] 本實施形態相關之化學機械研磨用組成物中之鉀以及鈉之含有比例，將鉀之含量設為MK （ppm），將鈉之含量設為MNa （ppm）時，MK /MNa 之值為3×103 ~3×105 較佳，為5×103 ~5×104 再較佳。MK /MNa 之值若在前述範圍內，則不會使半導體特性惡化，能夠進行化學機械研磨，同時於CMP步驟中能夠更有效地抑制露出於被研磨面之鈷被過度蝕刻並溶出，因此能夠維持安定之處理特性。 [0045] 本實施形態相關之化學機械研磨用組成物含有鈉1×10-6 ~1×101 ppm較佳，含有1×10-3 ~1×100 ppm再較佳。且，本實施形態相關之化學機械研磨用組成物含有鉀1×10-2 ~1×106 ppm較佳，含有1×10-1 ~1×105 ppm再較佳。 [0046] 為了使本實施形態相關之化學機械研磨用組成物含有鉀或鈉，添加水溶性之鉀鹽或鈉鹽即可。作為如此之水溶性之鹽，有舉例如鈉或鉀之氫氧化物、碳酸鹽、銨鹽、鹵化物等。 [0047] 且，本實施形態相關之化學機械研磨用組成物中含有的鉀之含量MK （ppm）以及鈉之含量MNa （ppm）能夠藉由使用ICP發光分析法（ICP-AES）、ICP質量分析法（ICP-MS）或原子吸光光度法（AA）定量化學機械研磨用組成物來求出。作為ICP發光分析裝置，能夠使用例如「ICPE-9000（股份公司島津製作所製）」等。作為ICP質量分析裝置，能夠使用例如「ICPM-8500（股份公司島津製作所製）」、「ELAN DRC PLUS（PerkinElmer公司製）」等。作為原子吸光分析裝置，能夠使用例如「AA-7000（股份公司島津製作所製）」、「ZA3000（股份公司日立Hightech Science）」等。 [0048] 且，本實施形態相關之化學機械研磨用組成物中含有的鉀以及鈉之含量能夠藉由將化學機械研磨用組成物以遠心分離將研磨粒去除，定量研磨粒以外之液狀介質中含有的鉀以及鈉來算出。因此，藉由將化學機械研磨用組成物以公知方法分析，能夠確認滿足本案發明之構成要件。 [0049] ＜防蝕劑＞ 本實施形態相關之化學機械研磨用組成物亦可含有防蝕劑。作為防蝕劑，有舉出苯並三唑、1,2,3-三唑、1,2,4-三唑以及此等之衍生物。防蝕劑之含量相對於化學機械研磨用組成物之全質量，較佳為1質量%以下，再較佳為0.001~0.1質量%。 [0050] 1.4.化學機械研磨用組成物之pH 本實施形態相關之化學機械研磨用組成物之pH較佳為7以上11以下，再較佳為8以上11以下，特別佳為9以上11以下。pH若在前述範圍內，則能夠一邊抑制鈷膜之腐蝕，一邊研磨鈷膜，因此能夠得到良好之研磨特性。另一方面，若pH未滿7，則鈷膜之研磨速度雖然會提升，但容易產生鈷膜之腐蝕，故難以得到良好之研磨特性。 [0051] 作為調整化學機械研磨用組成物之pH之手段，有舉例如於化學機械研磨用組成物中添加鹼基之方法。作為能夠添加之鹼基，有舉例如氨、氫氧化鉀、氫氧化鈉、TMAH（四甲基氫氧化銨）等。此等之鹼基，能夠單獨使用1種單獨或組合2種以上來使用。 [0052] 1.5.化學機械研磨用組成物之鈷之自然電位 本實施形態相關之化學機械研磨用組成物之鈷之自然電位為0~-500mV較佳，為-200~-500mV再較佳。化學機械研磨用組成物之鈷之自然電位若在前述範圍內，則於研磨步驟中，能夠抑制露出於被研磨面之鈷被過度蝕刻並溶出。相對於此，化學機械研磨用組成物中含有之化學機械研磨用組成物之鈷之自然電位超過前述範圍時，鈷變得容易氧化，化學上容易生成安定之氧化鈷或氫氧化鈷，難以有效率地來研磨，故較不佳。另一方面，化學機械研磨用組成物中含有之化學機械研磨用組成物之鈷之自然電位未滿前述範圍時，鈷之過度蝕刻會進行，被研磨面之平坦性或電氣特性有時會惡化。 [0053] 且，本案發明中，化學機械研磨用組成物之鈷之自然電位（穩定電位）能夠藉由定量化學機械研磨用組成物之開路電位（OCP）來求出。且，自然電位為腐蝕電位之同義詞，且能夠以線性掃描伏安法（LSV）並自塔菲爾圖定量腐蝕電位來求出。作為OCP以及LSV裝置，能夠使用例如「電氣化學測定裝置HZ-7000（北斗電工股份公司製）」等。 [0054] 1.6.化學機械研磨用水系分散體之表面張力 本實施形態相關之化學機械研磨用組成物之表面張力為20~75mN/m較佳，為50~75mN/m較佳。化學機械研磨用組成物之表面張力若在前述範圍內，則於研磨步驟中，能夠降低鈷表面之缺陷。 [0055] 化學機械研磨用組成物之表面張力能夠藉由增減上述具有一個以上雙鍵之陰離子性化合物或其他添加劑之添加量來調整。 [0056] 且，化學機械研磨用組成物之表面張力能夠藉由使用懸滴法（懸垂液滴法）定量化學機械研磨用組成物來求出。作為表面張力計，能夠使用例如「接觸角計DMs-401（協和界面科學股份公司製）」等。 [0057] 1.7.用途 本實施形態相關之化學機械研磨用組成物能夠達到如上述對鈷膜之實用上的研磨速度，並同時具有鈷膜之腐蝕抑制效果。因此，本實施形態相關之化學機械研磨用組成物在半導體裝置之製造步驟中，作為用來將形成金屬配線、金屬閘以及金屬插頭等之鈷膜進行化學機械研磨之研磨材料較適合。 [0058] 1.8.化學機械研磨用組成物之調製方法 本實施形態相關之化學機械研磨用組成物能夠藉由使上述各成分溶解或分散於水等之液狀介質中來調製。使其溶解或分散之方法並無特別限制，只要是能夠均勻地溶解或分散，亦可適用任何方法。且，關於上述各成分之混合順序或混合方法並無特別限制。 [0059] 且，本實施形態相關之化學機械研磨用組成物能夠作為濃縮型式的原液來調製，使用時再以水等之液狀介質稀釋使用。 [0060] 2.化學機械研磨方法 本發明之一實施形態相關之化學機械研磨方法包含使用上述化學機械研磨用組成物，將鈷膜進行化學機械研磨之步驟。以下，關於本實施形態相關之化學機械研磨方法之一具體例，一邊使用圖式一邊詳細地說明。 [0061] 2.1.裝置（被處理體）之製作 圖4表示本實施形態相關之化學機械研磨方法中所使用之被處理體100。 （1）首先，於矽基板（無圖示）上以電漿CVD法或熱氧化法形成絕緣膜20。作為絕緣膜20，有舉例如TEOS膜等。 （2）絕緣膜20上，使用CVD法或熱氧化法形成保護膜30。作為保護膜30，有舉例如SiN膜等。 （3）以絕緣膜20以及保護膜30連通之方式來蝕刻，形成配線用凹部40。 （4）使用CVD法或PVD法，形成障壁金屬膜50，使其被覆保護膜30之表面以及配線用凹部40之底部及內壁面。障壁金屬膜50，以與鈷膜之接著性以及對絕緣膜及保護膜之擴散障壁性優異之觀點來看，為Ti或TiN較佳，但不限於此等，亦可為Ta、TaN、Mn、Ru等。 （5）以PVD法、CVD法或鍍敷法使鈷堆積於障壁金屬膜50之上，形成鈷膜60，藉此得到被處理體100。 [0062] 2.2.化學機械研磨方法 接著，對被處理體100進行二階段的研磨處理。作為第1研磨處理步驟，為了去除堆積於被處理體100之障壁金屬膜50上的鈷膜60，使用特開2016-30831號公報等中記載之對鈷表示高研磨速率之化學機械研磨用組成物，來進行化學機械研磨。藉由此化學機械研磨，繼續研磨鈷膜60至保護膜30或障壁金屬膜50露出於表面為止。通常，確認到保護膜30或障壁金屬膜50露出於表面之後，必須要使研磨停止。雖然對鈷膜之研磨速度非常高，但使用幾乎不研磨障壁金屬膜之化學機械研磨用組成物時，如圖5所示，由於在障壁金屬膜50露出於表面之時點，無法進行化學機械研磨，故能夠使化學機械研磨自己停止（Self-stop）。 [0063] 接著，作為第2研磨處理步驟，藉由使用上述本案發明之化學機械研磨用組成物，研磨鈷膜60與障壁金屬膜50與保護膜30或絕緣膜20共存之被處理面，能夠使鈷膜表面之腐蝕降低，同時不會使研磨速度降低地研磨。 [0064] 2.3.化學機械研磨裝置 本實施形態相關之化學機械研磨方法中，能夠使用市售之化學機械研磨裝置。作為市售之化學機械研磨裝置，有舉例如荏原製作所公司製、型式「EPO-112」、「EPO-222」；Lapmaster SFT公司製、型式「LGP-510」、「LGP-552」；Applied Material公司製、型式「Mirra」、「Reflexion」；G&P TECHNOLOGY公司製、型式「POLI-400L」等。 [0065] 作為較佳研磨條件，應該要因所使用之化學機械研磨裝置來適當地設定，但例如作為化學機械研磨裝置使用上述「EPO-112」時，能夠設為下述條件。 ･定盤迴轉數；較佳為30~120rpm，再較佳為40~100rpm ･頭部迴轉數；較佳為30~120rpm，再較佳為40~100rpm ･定盤迴轉數/頭部迴轉數比；較佳為0.5~2，再較佳為0.7~1.5 ･研磨壓力；較佳為60~200gf/cm2 ，再較佳為100~ 150gf/cm2 ･化學機械研磨用組成物供給速度；較佳為50~300mL/分鐘，再較佳為100~200mL/分鐘 [0066] 3.實施例 以下，以本發明實施例來說明，但本發明並不限定於任何此等之實施例。且，本實施例之「份」以及「%」只要沒有特別限制，為質量基準。 [0067] 3.1.包含氫硫基修飾膠體二氧化矽之水分散體之調製 ＜二氧化矽粒子分散體A＞ 二氧化矽粒子分散體A如以下來製作。首先，混合扶桑化學工業公司製之高純度膠體二氧化矽（產品編號：PL-3；二氧化矽含量（固體成分濃度）20質量%，平均粒子徑75nm）5kg與3-硫氫基丙基三甲氧基矽氧烷6g，加熱還流2小時。如此，得到二氧化矽濃度為固體成分濃度20質量%，平均粒子徑72nm之亞磺醯化之二氧化矽粒子分散體A。 [0068] 將二氧化矽粒子分散體A以離子交換水稀釋至0.01%，1滴載於具有篩孔尺寸為150μm之Cu粒之膠棉膜上，於室溫下乾燥。如此，在Cu粒上不使粒子形狀崩解之狀態調製觀察用之樣品後，使用透過型電子顯微鏡（日立High-Technologies公司製，「H-7650」）以攝影倍率20000倍攝影粒子之影像，測定50個二氧化矽粒子之長徑以及短徑，算出其平均值。由長徑之平均值（Rmax）以及短徑之平均值（Rmin）算出其比（Rmax/Rmin）後，為1.2。 [0069] ＜二氧化矽粒子分散體B＞ 二氧化矽粒子分散體B如以下來製作。首先，混合扶桑化學工業公司製之高純度膠體二氧化矽（產品編號：PL-3L；二氧化矽含量（固體成分濃度）20質量%，平均粒子徑63nm）5kg與3-硫氫基丙基三甲氧基矽氧烷6g，加熱還流2小時。於此，得到二氧化矽濃度為固體成分濃度20質量%，平均二次粒子徑62nm之亞磺醯化之二氧化矽粒子分散體B。由長徑之平均值（Rmax）以及短徑之平均值（Rmin）算出其比（Rmax/Rmin）後，為1.1。 [0070] ＜二氧化矽粒子分散體C＞ 二氧化矽粒子分散體C如以下來製作。首先，混合扶桑化學工業公司製之高純度膠體二氧化矽（產品編號：PL-3；二氧化矽含量（固體成分濃度）20質量%，平均粒子徑75nm）5kg與3-胺基丙基三甲氧基矽氧烷6g，加熱還流2小時。如此，得到二氧化矽濃度為固體成分濃度20質量%，平均粒子徑73nm之胺化之二氧化矽粒子分散體C。由長徑之平均值（Rmax）以及短徑之平均值（Rmin）算出其比（Rmax/Rmin）後，為1.2。 [0071] ＜二氧化矽粒子分散體D＞ 二氧化矽粒子分散體D如以下來製作。首先，混合扶桑化學工業公司製之高純度膠體二氧化矽（產品編號：PL-3；二氧化矽含量（固體成分濃度）20質量%，平均粒子徑75nm）5kg與2-硝苄基酯6g，加熱還流2小時。之後，進行3小時光照射，得到二氧化矽濃度為固體成分濃度20質量%，平均粒子徑75nm之羧酸化之二氧化矽粒子分散體D。由長徑之平均值（Rmax）以及短徑之平均值（Rmin）算出其比（Rmax/Rmin）後，為1.2。 [0072] ＜二氧化矽粒子分散體E＞ 二氧化矽粒子分散體E如以下來製作。首先，混合扶桑化學工業公司製之高純度膠體二氧化矽（產品編號：PL-3；二氧化矽含量（固體成分濃度）20質量%，平均粒子徑75nm）5kg與3-硫氫基丙基三甲氧基矽氧烷6g，加熱還流2小時後，得到硫醇化二氧化矽溶膠。將其二氧化矽溶膠，藉由添加過氧化氫等之氧化劑並使其加熱還流8小時，使其表面氧化，磺酸固定化於表面。如此，得到二氧化矽濃度為固體成分濃度20質量%，平均粒子徑73nm二氧化矽粒子分散體E。由長徑之平均值（Rmax）以及短徑之平均值（Rmin）算出其比（Rmax/Rmin）後，為1.2。 [0073] 3.2.化學機械研磨用組成物之調製 於聚乙稀製容器中添加各成分，使其成為表1或表2所示之含有比例，進一步因應必要添加氫氧化鉀、氫氧化鈉、過氧化氫水，調整至表1或表2所示之pH、自然電位、鉀含量、鈉含量，來調製各實施例以及各比較例之化學機械研磨用組成物。 [0074] 3.3.評價方法 3.3.1.研磨速度評價 使用上述所調製之化學機械研磨用組成物，將附有直徑12吋之鈷膜200nm之晶圓作為被研磨體，以下述研磨條件進行1分鐘之化學機械研磨試驗。 [0075] ＜研磨條件＞ ･研磨裝置：G&P TECHNOLOGY公司製、型式「POLI-400L」 ･研磨墊片：富士紡績公司製、「多硬質聚氨基甲酸酯製墊片；H800-type1（3-1S）775」 ･化學機械研磨用組成物供給速度：100mL/分鐘 ･定盤迴轉數：100rpm ･頭部迴轉數：90rpm ･頭部按壓：2psi ･研磨速度（Å/min）=（研磨前之膜之厚度-研磨後之膜之厚度）/研磨時間 且，鈷膜之厚度藉由電阻率測定機（NPS公司製，型式「Σ-5」）並以直流4探針法來測定電阻，自此薄片電阻值與鈷之體積電阻率並藉由下述式來算出。 膜之厚度（Å）=[鈷膜之體積電阻率（Ω･m）÷薄片電阻值（Ω）]×1010 [0076] 研磨速度評價之評價基準如下述。將其結果合併表示於表1或表2。 ･研磨速度為400Å/min以上時，由於研磨速度較大，實際之半導體研磨中，能夠容易確保與其他材料膜之研磨之速度平衡，非常實用，故判斷為極良好，並表記為「◎」。 ･研磨速度200Å/min以上未滿400Å/min時，由於研磨速度較大，實際之半導體研磨中，能夠確保與其他材料膜之研磨之速度平衡，較實用，故判斷為良好，並表記為「○」。 ･研磨速度未滿200Å/min時，由於研磨速度較小，實用困難，判斷為不良，並表記為「×」。 [0077] 3.3.2.腐蝕評價 切斷上述研磨速度評價所研磨之附有直徑12吋之鈷膜之晶圓，製作2×2cm之試驗片，以掃描型原子力顯微鏡（Bluker Corpoation製，AFM）使用Dimension FastScan，於框大小10μm觀察12處，算出12處之算術平均粗度之平均值。其評價基準如下述。將其結果合併表示於表1或表2。 ･算術平均粗度之平均值未滿0.6nm時，能夠抑制鈷腐蝕，判斷為非常良好，並表記為「○」。 ･算術平均粗度之平均值為0.6nm以上時，無法抑制鈷腐蝕，使用困難，故判斷為不良，並表記為「×」。 [0078][0079][0080] 表1以及表2中，各實施例以及各比較例中的各成分之合計量為100質量份，殘於部分為離子交換水。且，補足關於表1以及表2之下述成分。 ＜研磨粒＞ ･PL-3：扶桑化學工業公司製，商品名「PL-3」、Rmax /Rmin=1.2 ･PL-3L：扶桑化學工業公司製，商品名「PL-3L」、Rmax /Rmin=1.2 [0081] 3.4.評價結果 藉由實施例1~9之本案發明相關之化學機械研磨用組成物，能夠將鈷膜以高研磨速度研磨，另一方面，研磨後之鈷膜之表面粗度較低，為低腐蝕，儲藏安定性之結果也較良好。另一方面，比較例1~5之化學機械研磨用組成物，能夠使鈷膜之腐蝕抑制與鈷膜之高研磨速度兩立，無法得到良好之研磨特性。 [0082] 本發明並不限定於上述實施形態，能夠為各種變形。例如，本發明包含與實施形態所說明之構成實質上相同之構成（例如機能、方法以及結果相同之構成或目的以及效果相同之構成）。且，本發明包含取代實施形態所說明之構成之非本質的部分之構成。且，本發明包含達到與實施形態所說明之構成相同作用效果之構成或能夠達成相同目的之構成。且，本發明包含在實施形態所說明之構成中附加公知技術之構成。[Mode for Carrying Out the Invention] [0019] Hereinafter, suitable embodiments of the present invention will be described in detail. In addition, the present invention is not limited to the embodiments described below, and various modifications may be included without departing from the gist of the present invention. 1. Composition for Chemical Mechanical Polishing A composition for chemical mechanical polishing according to an embodiment of the present invention is characterized in that it contains abrasive particles and a liquid medium containing hydrogen-sulfur groups which are immobilized on the surface through a covalent bond. . Hereinafter, the chemical mechanical polishing composition according to this embodiment will be described in detail. [0021] 1.1. Abrasive particles The chemical mechanical polishing composition according to this embodiment contains abrasive particles having a hydrogen sulfide group (-SH) immobilized on the surface through covalent bonding. Since the abrasive grains used in this embodiment are abrasive grains having a hydrogen-sulfur group fixed on the surface via a covalent bond, they do not include abrasives that are physically or ionicly adsorbed if a compound having a hydrogen-sulfur group on the surface is used. grain. [0022] The material of the abrasive particles used in this embodiment is not particularly limited, and examples thereof include silicon dioxide, cerium dioxide, aluminum oxide, zirconium dioxide, and titanium oxide, but silicon dioxide is preferred. Hydrogen sulfide (-SH) silicon dioxide particles immobilized on the surface via a covalent bond can be produced, for example, as follows. [0023] First, silicon dioxide particles are prepared. Examples of the silica particles include fumed silica, colloidal silica, and the like, but colloidal silica is preferred from the viewpoint of reducing abrasive defects such as scratches. As the colloidal silicon dioxide, those produced by a method described in, for example, Japanese Patent Application Laid-Open No. 2003-109921 can be used. [0024] The surface modification of the silicon dioxide particles can be applied to the method described in Japanese Patent Application Laid-Open No. 2010-269985 or J. Ind. Eng. Chem., Vol. 12, No. 6, (2006) 911-917 and the like. Specifically, it can be produced by sufficiently stirring the silicon dioxide particles and the hydrogen sulfide-containing siloxane coupling agent in an acidic medium, so that the hydrogen sulfide-containing siloxane coupling agent is covalently bonded to The surface of the silica particles. Examples of the hydrosulfan-containing siloxane coupling agent include 3-thiohydropropylmethyldimethoxysiloxane and 3-thiohydropropyltrimethoxysiloxane. [0025] The silicon dioxide particles thus obtained are immobilized on the surface through a hydrogen-sulfur group via a covalent bond. Therefore, in the chemical mechanical polishing composition, the surface of the silicon dioxide particles is negatively charged by the functional group, and the silicon dioxide particles become easily adsorbed on the surface of the cobalt film. As a result, since the silicon dioxide particles are localized on the surface of the cobalt film, the mechanical polishing force is increased, and the polishing speed of the cobalt film is also increased. [0026] The surface potential (Zeta potential) of the abrasive grains is a negative potential in a region where the pH of the chemical mechanical polishing composition is 7 or more and 11 or less, and its negative potential is preferably −20 mV or less. If the Zeta potential is -20 mV or less, as described above, the abrasive particles will easily adhere to the surface of the cobalt film, so the polishing speed of the cobalt film will be increased. Examples of Zeta potential measuring devices include "ELSZ-1" manufactured by Otsuka Electronics Co., Ltd., and "Zetasizer nanozs" manufactured by Malvern. The Zeta potential of the abrasive grains can be appropriately adjusted by increasing or decreasing the addition amount of the hydrogen-sulfur group-containing siloxane coupling agent. [0027] The average particle diameter of the abrasive particles can be determined by measuring with a particle size distribution measuring device using a dynamic light scattering method as a measuring principle. The average particle diameter of the abrasive particles is preferably 15 nm to 100 nm, more preferably 20 nm to 80 nm, and particularly preferably 30 nm to 70 nm. If the average particle diameter of the abrasive grains is within the aforementioned range, a chemical mechanical polishing composition having a practical polishing rate for a cobalt film, which is difficult to cause sedimentation and separation of the abrasive grains, and excellent storage stability, can be obtained. Examples of particle size distribution measurement devices that use the dynamic light scattering method as the measuring principle include the Nano particle analyzer "DelsaNano S" manufactured by Beckman Coulter; "Zetasizer nano zs" manufactured by Malvern; manufactured by Horiba Manufacturing Co., Ltd. "LB550" and so on. In addition, the average particle diameter measured by the dynamic light scattering method indicates the average particle diameter of secondary particles formed by aggregating a plurality of primary particles. [0028] The ratio Rmax / Rmin of the long diameter (Rmax) and the short diameter (Rmin) of the abrasive particles is preferably 1.0 to 1.5, more preferably 1.0 to 1.4, and particularly preferably 1.0 to 1.3. When Rmax / Rmin is within the above range, a defect of the cobalt film to be polished is not caused, and high polishing speed and high planarization characteristics can be achieved at the same time. [0029] Here, the long diameter (Rmax) of the abrasive particles refers to the distance between the end of the image and the longest straight line among the lines of an image of an independent abrasive particle photographed with a transmission electron microscope. The short diameter (Rmin) of the abrasive particles refers to the distance between the end of the image and the shortest straight line among the images of an independent abrasive particle photographed by a transmission electron microscope. [0030] For example, as shown in FIG. 1, when an image of an independent abrasive particle 10 a photographed by a transmission electron microscope is elliptical, the major axis a of the elliptical shape is determined as the major diameter (Rmax) of the abrasive particle. , The minor axis b is determined as the minor diameter (Rmin) of the abrasive particles. As shown in FIG. 2, when an image of an independent abrasive particle 10 b taken by a transmission electron microscope is an aggregate of two primary particles, the longest distance c between a straight line connecting the end of the image and the end is determined as The longest diameter (Rmax) of the abrasive grains is determined as the shortest diameter (Rmin) of the abrasive grains in the shortest diameter d of the straight line connecting the end portion of the image and the end portion. As shown in Fig. 3, when the image of an independent abrasive particle 10c taken by a transmission electron microscope is an aggregate of three or more primary particles, the longest distance e in the straight line connecting the end portion of the image and the end portion is determined. The longest diameter (Rmax) of the abrasive grains is determined as the shortest diameter (Rmin) of the abrasive grains in the shortest diameter f of the straight line connecting the end portion of the image and the end portion. [0031] With the above-mentioned method of judgment, for example, the long diameter (Rmax) and short diameter (Rmin) of 50 abrasive particles can be measured, the average of the long diameter (Rmax) and the short diameter (Rmin) can be calculated, and then borrowed. It is calculated by calculating the ratio (Rmax / Rmin) of the average value of the long diameter to the average value of the short diameter. [0032] The content of the abrasive grains is preferably 1 to 20% by mass, more preferably 1 to 15% by mass, and particularly preferably 1 to 10% by mass relative to the total mass of the chemical mechanical polishing composition. If the content ratio of the abrasive grains is within the aforementioned range, a sufficient polishing rate for the cobalt film can be obtained, and the dispersion stability of the abrasive grains in the composition for chemical mechanical polishing is good. [0033] 1.2. Liquid medium The chemical mechanical polishing composition according to this embodiment contains a liquid medium. Examples of the liquid medium include water, a mixed medium of water and ethanol, and a mixed medium containing water and an organic solvent having compatibility with water. Among these, a mixed medium using water, water, and ethanol is preferred, and water is more preferred. [0034] 1.3 Other Components The chemical mechanical polishing composition according to this embodiment can contain an anionic compound having one or more double bonds, potassium and sodium, an anticorrosive agent, Japanese Patent Application Laid-Open No. 2014-229827, etc., in addition to the above components. Additives such as the well-known organic acids (except for anionic compounds having more than one double bond), surfactants, and the like. [0035] <Anionic compound having one or more double bonds> The chemical mechanical polishing composition according to this embodiment preferably contains an anionic compound having one or more double bonds. Such an anionic compound can chelate with cobalt atoms on the surface of the modified cobalt film. As a result, cobalt is dissolved in the composition for chemical mechanical polishing, and the polishing speed of the cobalt film may be increased in some cases. [0036] As the anionic compound having one or more double bonds, a compound represented by the following general formulae (1) to (3) is more preferred. [0037] (In the above general formula (1), R 1 is an alkyl group or carboxyl group having 1 to 8 carbon atoms, and R 2 represents an organic group or carboxyl group having 1 to 15 carbon atoms.) [0038] [0039] [0040] In the general formula (2) and the general formula (3), R 3 , R 4 , R 5, and R 6 each independently represent hydrogen or an organic group having a carbon number of 1 to 3 or a carboxyl group. However, at least one of R 3 and R 4 represents an organic group or carboxyl group having a carbon number of 1 to 3, and at least one of R 5 and R 6 represents an organic group or a carboxyl group having a carbon number of 1 to 3. [0041] Specific examples of the anionic compound having one or more double bonds include, for example, maleic acid, butenedioic acid, quinolinic acid, quinaldic acid, oleic acid, alkenyl succinic acid, and salts thereof. One or more of these can be used. [0042] The content of the anionic compound having one or more double bonds is preferably 0.0001 to 1% by mass, and more preferably 0.001 to 0.5% by mass, relative to the total mass of the chemical mechanical polishing composition. If the content ratio of the anionic compound having more than one double bond is within the aforementioned range, the corrosion of the cobalt film can be suppressed, and the polishing speed of the cobalt film will be increased. [0043] <Potassium and Sodium> The chemical mechanical polishing composition according to the embodiment preferably contains potassium and sodium. Generally, as described in Japanese Patent Application Laid-Open No. 2000-208451, alkali metals such as sodium or potassium are considered as impurities that should be removed as much as possible in the manufacturing process of semiconductors. Therefore, among various compositions used in semiconductor processing of chemical mechanical polishing compositions, etc., as the base for controlling pH, it is not an inorganic base such as sodium hydroxide, and tetramethylammonium hydroxide (TMAH) is used. Other organic bases are preferred. However, in the present invention, in the polishing step, the use of a chemical mechanical polishing composition containing potassium and sodium in a specific ratio does not significantly degrade the semiconductor characteristics, but has the effect of improving the processing characteristics. [0044] The content ratio of potassium and sodium in the chemical-mechanical polishing composition according to this embodiment, the content of potassium is set to M K (ppm), and the content of sodium is set to M Na (ppm), M K The value of / M Na is preferably 3 × 10 3 to 3 × 10 5, and more preferably 5 × 10 3 to 5 × 10 4 . If the value of M K / M Na is within the aforementioned range, the semiconductor characteristics will not be deteriorated, chemical mechanical polishing can be performed, and at the same time, the cobalt exposed on the surface to be polished can be more effectively suppressed from being excessively etched and eluted in the CMP step. Therefore, stable processing characteristics can be maintained. [0045] The chemical mechanical polishing composition according to this embodiment preferably contains sodium 1 × 10 −6 to 1 × 10 1 ppm, and more preferably contains 1 × 10 −3 to 1 × 10 0 ppm. In addition, the chemical mechanical polishing composition according to this embodiment preferably contains potassium 1 × 10 -2 to 1 × 10 6 ppm, and more preferably contains 1 × 10 -1 to 1 × 10 5 ppm. [0046] In order that the chemical mechanical polishing composition according to this embodiment contains potassium or sodium, a water-soluble potassium salt or sodium salt may be added. Examples of such water-soluble salts include hydroxides, carbonates, ammonium salts, and halides of sodium or potassium. [0047] In addition, the content of potassium M K (ppm) and the content of sodium M Na (ppm) contained in the chemical-mechanical polishing composition according to this embodiment can be obtained by using an ICP emission analysis method (ICP-AES), ICP mass analysis (ICP-MS) or atomic absorption spectrometry (AA) was used to quantify the composition for chemical mechanical polishing. As the ICP emission analysis device, for example, "ICPE-9000 (manufactured by Shimadzu Corporation)" can be used. As the ICP mass analysis device, for example, "ICPM-8500 (manufactured by Shimadzu Corporation)", "ELAN DRC PLUS (manufactured by PerkinElmer)", and the like can be used. As the atomic absorption analysis device, for example, “AA-7000 (manufactured by Shimadzu Corporation)”, “ZA3000 (Hitachi Hightech Science Corporation)”, and the like can be used. [0048] In addition, the content of potassium and sodium contained in the chemical mechanical polishing composition according to this embodiment can be removed by telecentric separation of the chemical mechanical polishing composition, and the liquid medium other than the abrasive particles can be quantified. The content of potassium and sodium is calculated. Therefore, by analyzing the chemical mechanical polishing composition by a known method, it can be confirmed that the constitutional requirements of the present invention are satisfied. [0049] <Anticorrosive Agent> The chemical mechanical polishing composition according to this embodiment may further include an anticorrosive agent. Examples of the corrosion inhibitor include benzotriazole, 1,2,3-triazole, 1,2,4-triazole, and derivatives thereof. The content of the corrosion inhibitor is preferably 1% by mass or less, and more preferably 0.001 to 0.1% by mass, relative to the total mass of the chemical mechanical polishing composition. 1.4. PH of the composition for chemical mechanical polishing The pH of the composition for chemical mechanical polishing according to this embodiment is preferably 7 or more and 11 or less, still more preferably 8 or more and 11 or less, and particularly preferably 9 or more and 11 or less . When the pH is within the above range, the cobalt film can be polished while suppressing the corrosion of the cobalt film, and thus good polishing characteristics can be obtained. On the other hand, if the pH is less than 7, although the polishing speed of the cobalt film is increased, corrosion of the cobalt film is likely to occur, so it is difficult to obtain good polishing characteristics. [0051] As a means for adjusting the pH of the composition for chemical mechanical polishing, for example, a method of adding a base to the composition for chemical mechanical polishing is mentioned. Examples of bases that can be added include ammonia, potassium hydroxide, sodium hydroxide, TMAH (tetramethylammonium hydroxide), and the like. These bases can be used singly or in combination of two or more kinds. [0052] 1.5 Natural potential of cobalt of chemical mechanical polishing composition The natural potential of cobalt of the chemical mechanical polishing composition according to this embodiment is preferably 0 to -500 mV, more preferably -200 to -500 mV. If the natural potential of cobalt in the chemical mechanical polishing composition is within the aforementioned range, in the polishing step, the cobalt exposed on the surface to be polished can be suppressed from being excessively etched and eluted. On the other hand, when the natural potential of cobalt contained in the chemical mechanical polishing composition contained in the chemical mechanical polishing composition exceeds the foregoing range, cobalt becomes easily oxidized, and stable cobalt oxide or cobalt hydroxide is easily formed chemically. It is not good to grind efficiently. On the other hand, if the natural potential of cobalt contained in the chemical mechanical polishing composition contained in the chemical mechanical polishing composition is less than the aforementioned range, excessive etching of cobalt may occur, and the flatness or electrical characteristics of the polished surface may deteriorate. . [0053] In the present invention, the natural potential (stable potential) of cobalt of the chemical mechanical polishing composition can be determined by quantifying the open circuit potential (OCP) of the chemical mechanical polishing composition. In addition, the natural potential is synonymous with the corrosion potential, and can be determined by linear scanning voltammetry (LSV) and quantifying the corrosion potential from a Tafel diagram. As the OCP and LSV devices, for example, "electrochemical measurement device HZ-7000 (manufactured by Hokuto Denko Corporation)" can be used. [0054] 1.6. Surface tension of the chemical mechanical polishing aqueous dispersion The surface tension of the chemical mechanical polishing composition according to this embodiment is preferably 20 to 75 mN / m, and more preferably 50 to 75 mN / m. If the surface tension of the chemical mechanical polishing composition is within the aforementioned range, defects on the cobalt surface can be reduced in the polishing step. [0055] The surface tension of the composition for chemical mechanical polishing can be adjusted by increasing or decreasing the amount of the above-mentioned anionic compound having one or more double bonds or other additives. [0056] The surface tension of the composition for chemical mechanical polishing can be determined by quantifying the composition for chemical mechanical polishing using a hanging drop method (drape droplet method). As the surface tensiometer, for example, "contact angle meter DMs-401 (made by Kyowa Interface Science Co., Ltd.)" can be used. [0057] 1.7 Use The chemical mechanical polishing composition according to this embodiment can achieve the practical polishing speed for the cobalt film as described above, and at the same time, it has the effect of inhibiting the corrosion of the cobalt film. Therefore, the chemical-mechanical polishing composition according to this embodiment is suitable as a polishing material for chemical-mechanical polishing of a cobalt film forming a metal wiring, a metal gate, a metal plug, and the like in a manufacturing process of a semiconductor device. [0058] 1.8. Method for preparing chemical mechanical polishing composition The chemical mechanical polishing composition according to this embodiment can be prepared by dissolving or dispersing the above components in a liquid medium such as water. The method of dissolving or dispersing is not particularly limited, and any method can be applied as long as it can dissolve or disperse uniformly. In addition, there is no particular limitation on the mixing order or mixing method of the above-mentioned components. [0059] In addition, the chemical mechanical polishing composition according to this embodiment can be prepared as a concentrated type stock solution, and when used, it can be diluted with a liquid medium such as water and used. 2. Chemical-mechanical polishing method A chemical-mechanical polishing method according to an embodiment of the present invention includes a step of chemical-mechanical polishing a cobalt film using the above-mentioned chemical mechanical polishing composition. Hereinafter, a specific example of the chemical mechanical polishing method according to this embodiment will be described in detail while using drawings. [0061] 2.1. Production of Apparatus (Subject) FIG. 4 shows the subject 100 used in the chemical mechanical polishing method according to this embodiment. (1) First, an insulating film 20 is formed on a silicon substrate (not shown) by a plasma CVD method or a thermal oxidation method. Examples of the insulating film 20 include a TEOS film and the like. (2) A protective film 30 is formed on the insulating film 20 using a CVD method or a thermal oxidation method. Examples of the protective film 30 include a SiN film. (3) Etching is performed so that the insulating film 20 and the protective film 30 communicate with each other to form a wiring recess 40. (4) The barrier metal film 50 is formed using a CVD method or a PVD method, and covers the surface of the protective film 30 and the bottom and inner wall surfaces of the wiring recess 40. The barrier metal film 50 is preferably Ti or TiN from the viewpoint of excellent adhesion to a cobalt film and excellent diffusion barrier properties to an insulating film and a protective film, but is not limited to these, and may be Ta, TaN, Mn , Ru, etc. (5) Cobalt is deposited on the barrier metal film 50 by a PVD method, a CVD method, or a plating method to form a cobalt film 60, thereby obtaining the object 100 to be processed. [0062] 2.2. Chemical Mechanical Polishing Method Next, the object 100 is subjected to a two-stage polishing process. As a first polishing treatment step, in order to remove the cobalt film 60 deposited on the barrier metal film 50 of the object 100, a chemical mechanical polishing composition described in JP 2016-30831 and the like that shows a high polishing rate for cobalt is used. For chemical mechanical polishing. By this chemical mechanical polishing, the cobalt film 60 is continuously polished until the protective film 30 or the barrier metal film 50 is exposed on the surface. Generally, after confirming that the protective film 30 or the barrier metal film 50 is exposed on the surface, it is necessary to stop polishing. Although the polishing speed of the cobalt film is very high, when a chemical mechanical polishing composition that hardly polishes the barrier metal film is used, as shown in FIG. 5, chemical mechanical polishing cannot be performed at the time when the barrier metal film 50 is exposed on the surface. , So it can make the chemical mechanical grinding self-stop. [0063] Next, as the second polishing processing step, by using the chemical mechanical polishing composition of the invention of the present invention, the surface to be processed where the cobalt film 60, the barrier metal film 50, the protective film 30 or the insulating film 20 coexist can be polished, It reduces the corrosion of the surface of the cobalt film, and does not reduce the polishing speed. [0064] 2.3. Chemical Mechanical Polishing Device In the chemical mechanical polishing method according to this embodiment, a commercially available chemical mechanical polishing device can be used. Commercially available chemical mechanical polishing devices include, for example, the types "EPO-112" and "EPO-222" made by Ebara Corporation; the types "LGP-510" and "LGP-552" made by Lapmaster SFT; Applied Material Company system, model "Mirra", "Reflexion"; G & P TECHNOLOGY company system, model "POLI-400L", etc. [0065] The preferred polishing conditions should be appropriately set depending on the chemical mechanical polishing device used. For example, when the above-mentioned "EPO-112" is used as a chemical mechanical polishing device, the following conditions can be set. ･ Fixed number of rotations of the plate; preferably 30 ~ 120rpm, more preferably 40 ~ 100rpm 数 Number of times of rotation of the head; preferably 30 ~ 120rpm, even more preferably 40 ~ 100rpm Ratio; preferably 0.5 ~ 2, still more preferably 0.7 ~ 1.5 ･ grinding pressure; preferably 60 ~ 200gf / cm 2 , still more preferably 100 ~ 150gf / cm 2 ･ chemical mechanical polishing composition supply speed; It is preferably 50 to 300 mL / min, and still more preferably 100 to 200 mL / min. [0066] 3. Examples Hereinafter, the examples of the present invention will be described, but the present invention is not limited to any of these examples. In addition, "part" and "%" in this embodiment are quality standards as long as there are no particular restrictions. [0067] 3.1. Preparation of an aqueous dispersion containing hydrogen-sulfur-modified colloidal silicon dioxide <silica dioxide particle dispersion A> The silicon dioxide particle dispersion A was prepared as follows. First, 5 kg of high-purity colloidal silicon dioxide (product number: PL-3; silicon dioxide content (solid content concentration) 20% by mass, average particle diameter 75nm) manufactured by Fuso Chemical Industry Co., Ltd. were mixed with 3-thiohydropropyl group 6 g of trimethoxysilyl was heated for 2 hours. In this manner, a sulfinated silicon dioxide particle dispersion A having a silicon dioxide concentration of 20% by mass as a solid content concentration and an average particle diameter of 72 nm was obtained. [0068] The silicon dioxide particle dispersion A was diluted to 0.01% with ion-exchanged water, and 1 drop was loaded on a cotton wool film having Cu particles with a mesh size of 150 μm, and dried at room temperature. In this way, after preparing the observation sample on the Cu particles without disintegrating the particle shape, a transmission electron microscope (H-7650, manufactured by Hitachi High-Technologies, Inc.) was used to photograph the particles at a magnification of 20,000 times. The long and short diameters of 50 silica particles were measured, and the average value was calculated. The ratio (Rmax / Rmin) was calculated from the average value (Rmax) of the long diameter and the average value (Rmin) of the short diameter, and was 1.2. [0069] <Silicon Dioxide Particle Dispersion B> The silicon dioxide particle dispersion B is prepared as follows. First, 5 kg of high-purity colloidal silicon dioxide (product number: PL-3L; silicon dioxide content (solid content concentration) 20% by mass, average particle diameter 63nm) manufactured by Fuso Chemical Industry Co., Ltd. were mixed with 3-thiohydropropyl group. 6 g of trimethoxysilyl was heated for 2 hours. Here, a sulfinated silicon dioxide particle dispersion B having a silicon dioxide concentration of 20% by mass as a solid content concentration and an average secondary particle diameter of 62 nm was obtained. The ratio (Rmax / Rmin) was calculated from the average value (Rmax) of the long diameter and the average value (Rmin) of the short diameter, and it was 1.1. [0070] <Silica Dioxide Particle Dispersion C> The silicon dioxide particle dispersion C is prepared as follows. First, 5 kg of high-purity colloidal silicon dioxide (product number: PL-3; silicon dioxide content (solid content concentration) 20% by mass, average particle diameter 75nm) manufactured by Fuso Chemical Industry Co., Ltd. were mixed with 3-aminopropyltrimethyl 6 g of oxysiloxane was heated for 2 hours. Thus, an aminated silicon dioxide particle dispersion C having a silicon dioxide concentration of 20% by mass as a solid content concentration and an average particle diameter of 73 nm was obtained. The ratio (Rmax / Rmin) was calculated from the average value (Rmax) of the long diameter and the average value (Rmin) of the short diameter, and was 1.2. [0071] <Silica Dioxide Particle Dispersion D> The silicon dioxide particle dispersion D is prepared as follows. First, 5 kg of high-purity colloidal silicon dioxide (product number: PL-3; silicon dioxide content (solid content concentration) 20% by mass, average particle diameter 75nm) manufactured by Fuso Chemical Industry Co., Ltd. were mixed with 6 g of 2-nitrobenzyl ester , Heating also flow for 2 hours. Thereafter, light irradiation was performed for 3 hours to obtain a carboxylated silicon dioxide particle dispersion D having a silicon dioxide concentration of 20% by mass as a solid content concentration and an average particle diameter of 75 nm. The ratio (Rmax / Rmin) was calculated from the average value (Rmax) of the long diameter and the average value (Rmin) of the short diameter, and was 1.2. [0072] <Silica Dioxide Particle Dispersion E> The silicon dioxide particle dispersion E is prepared as follows. First, 5 kg of high-purity colloidal silicon dioxide (product number: PL-3; silicon dioxide content (solid content concentration) 20% by mass, average particle diameter 75nm) manufactured by Fuso Chemical Industry Co., Ltd. were mixed with 3-thiohydropropyl group 6 g of trimethoxysiloxane was heated and flowed for 2 hours to obtain a thiolated silica dioxide sol. The surface of the silica sol was oxidized by adding an oxidant such as hydrogen peroxide and heating for 8 hours to oxidize the surface, and the sulfonic acid was immobilized on the surface. In this manner, a silicon dioxide particle dispersion E having a silicon dioxide concentration of 20% by mass as a solid content concentration and an average particle diameter of 73 nm was obtained. The ratio (Rmax / Rmin) was calculated from the average value (Rmax) of the long diameter and the average value (Rmin) of the short diameter, and was 1.2. [0073] 3.2 Preparation of Chemical Mechanical Polishing Composition Each component is added to a polyethylene container so as to have the content ratio shown in Table 1 or Table 2. Further, potassium hydroxide, sodium hydroxide, Hydrogen peroxide water was adjusted to the pH, natural potential, potassium content, and sodium content shown in Table 1 or Table 2 to prepare the chemical mechanical polishing composition of each example and each comparative example. 3.3. Evaluation method 3.3.1. Evaluation of polishing rate Using the chemical mechanical polishing composition prepared above, a wafer with a diameter of 200 nm and a cobalt film with a diameter of 12 inches was used as an object to be polished, and the following polishing conditions were performed. Chemical mechanical polishing test in minutes. [Polishing conditions] ･ Grinding device: G & P TECHNOLOGY company, type "POLI-400L" ･ Grinding pad: Fuji Textile Corporation, "multi-rigid polyurethane pad; H800-type1 (3- 1S) 775 ″ 供给 Feeding speed of chemical mechanical polishing composition: 100mL / min ･ Number of plate rotations: 100rpm 数 Number of head rotations: 90rpm ･ Head pressing: 2psi ･ Grinding speed (Å / min) = (Before grinding Thickness of film-thickness of film after polishing) / grinding time The thickness of the cobalt film was measured by a resistivity measuring machine (manufactured by NPS Corporation, type "Σ-5") using a DC 4-probe method. This sheet resistance value and the volume resistivity of cobalt are calculated by the following formula. Film thickness (Å) = [Volume resistivity of the cobalt film (Ω ･ m) ÷ sheet resistance value (Ω)] × 10 10 [0076] The evaluation criteria of the polishing rate evaluation are as follows. The results are combined and shown in Table 1 or Table 2. ･ When the polishing speed is 400Å / min or more, the polishing speed is large. In actual semiconductor polishing, it is easy to ensure the speed balance with the polishing of other material films. It is very practical, so it is judged to be very good. . ･ When the grinding speed is 200Å / min or more and less than 400Å / min, the grinding speed is large. In actual semiconductor grinding, the speed of grinding with other material films can be balanced, which is more practical. Therefore, it is judged to be good. ○ ". ･ When the grinding speed is less than 200 Å / min, the grinding speed is small and it is difficult to be practical, so it is judged as defective, and it is marked as "×". [0077] 3.3.2. Corrosion Evaluation The wafer with a cobalt film having a diameter of 12 inches polished by the above-mentioned polishing rate evaluation was cut, a 2 × 2 cm test piece was produced, and a scanning atomic force microscope (Bluker Corpoation, AFM) was used. Using Dimension FastScan, observe 12 points at a frame size of 10 μm, and calculate the average of the arithmetic mean thickness of the 12 points. The evaluation criteria are as follows. The results are combined and shown in Table 1 or Table 2.时 When the average value of the arithmetic mean thickness is less than 0.6 nm, cobalt corrosion can be suppressed, and it is judged to be very good, and it is expressed as "○".时 When the average of the arithmetic mean thickness is 0.6 nm or more, cobalt corrosion cannot be suppressed, and it is difficult to use. Therefore, it is judged to be bad, and it is expressed as "×". [0078] [0079] [0080] In Tables 1 and 2, the total amount of each component in each example and each comparative example was 100 parts by mass, and the remainder was ion-exchanged water. In addition, the following components regarding Tables 1 and 2 are supplemented. <Grinding particles> ･ PL-3: Made by Fuso Chemical Industry Co., Ltd. under the trade name "PL-3", Rmax / Rmin = 1.2 ･ PL-3L: Made by Fuso Chemical Industry Co., Ltd. under the trade name "PL-3L", Rmax / Rmin = 1.2 [0081] 3.4. Evaluation Results By using the chemical mechanical polishing composition related to the invention of Examples 1 to 9, the cobalt film can be polished at a high polishing rate. On the other hand, the surface of the polished cobalt film is coarse. The degree of corrosion is low, the result is low corrosion, and the storage stability results are also good. On the other hand, in the chemical mechanical polishing compositions of Comparative Examples 1 to 5, the corrosion suppression of the cobalt film and the high polishing rate of the cobalt film could be balanced, and good polishing characteristics could not be obtained. [0082] The present invention is not limited to the embodiment described above, and various modifications are possible. For example, the present invention includes a configuration substantially the same as the configuration described in the embodiment (for example, a configuration having the same function, method, and result, or a configuration having the same purpose and effect). The present invention includes a configuration that replaces the non-essential part of the configuration described in the embodiment. In addition, the present invention includes a configuration that achieves the same effect as the configuration described in the embodiment or a configuration that can achieve the same purpose. The present invention includes a configuration in which a known technique is added to the configuration described in the embodiment.
[0083][0083]
10a、10b、10c‧‧‧研磨粒10a, 10b, 10c‧‧‧ abrasive
20‧‧‧絕緣膜20‧‧‧ insulating film
30‧‧‧保護膜30‧‧‧ protective film
40‧‧‧配線用凹部40‧‧‧ Recess for wiring
50‧‧‧障壁金屬膜50‧‧‧ barrier metal film
60‧‧‧鈷膜60‧‧‧Cobalt film
100‧‧‧被處理體100‧‧‧ object
[0018] [圖1] 將研磨粒之長徑以及短徑之概念模式性地表示之說明圖。 [圖2] 將研磨粒之長徑以及短徑之概念模式性地表示之說明圖。 [圖3] 將研磨粒之長徑以及短徑之概念模式性地表示之說明圖。 [圖4] 將本實施形態之化學機械研磨方法中所使用之被處理體模式性地表示之剖面圖。 [圖5] 用來說明本實施形態之化學機械研磨方法之研磨步驟之剖面圖。[0018] [FIG. 1] An explanatory diagram schematically showing the concepts of the major and minor diameters of the abrasive grains. [Fig. 2] An explanatory diagram schematically showing the concepts of the major and minor diameters of the abrasive grains. [Fig. 3] An explanatory diagram schematically showing the concepts of the major and minor diameters of the abrasive grains. [Fig. 4] A cross-sectional view schematically showing an object to be processed used in the chemical mechanical polishing method of this embodiment. [Fig. 5] A cross-sectional view for explaining the polishing steps of the chemical mechanical polishing method of this embodiment.
Claims (7)
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| JP7159881B2 (en) * | 2019-01-17 | 2022-10-25 | Jsr株式会社 | Chemical mechanical polishing aqueous dispersion and chemical mechanical polishing method |
| WO2020255581A1 (en) * | 2019-06-20 | 2020-12-24 | 富士フイルム株式会社 | Polishing fluid and chemical mechanical polishing method |
| WO2022004197A1 (en) * | 2020-06-30 | 2022-01-06 | Jsr株式会社 | Method for manufacturing abrasive grains, composition for chemical mechanical polishing and method for chemical mechanical polishing |
| KR20230029618A (en) * | 2020-06-30 | 2023-03-03 | 제이에스알 가부시끼가이샤 | Method for producing abrasive particles, chemical mechanical polishing composition and chemical mechanical polishing method |
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| JP3804009B2 (en) * | 2001-10-01 | 2006-08-02 | 触媒化成工業株式会社 | Silica particle dispersion for polishing, method for producing the same, and abrasive |
| JP2006147993A (en) * | 2004-11-24 | 2006-06-08 | Hitachi Chem Co Ltd | Polishing solution for cmp and polishing method |
| JP2007194593A (en) * | 2005-12-20 | 2007-08-02 | Fujifilm Corp | Polishing liquid for metal and polishing method using the same |
| KR101562416B1 (en) * | 2008-02-06 | 2015-10-21 | 제이에스알 가부시끼가이샤 | Aqueous dispersion for chemical mechanical polishing and chemical mechanical polishing method |
| JP2010041027A (en) * | 2008-02-18 | 2010-02-18 | Jsr Corp | Aqueous dispersion for chemical mechanical polishing and method of manufacturing the same, and chemical mechanical polishing method |
| JP4580433B2 (en) * | 2008-04-14 | 2010-11-10 | 野村マイクロ・サイエンス株式会社 | Method for regenerating polishing slurry |
| JP6028432B2 (en) * | 2012-07-17 | 2016-11-16 | 日立化成株式会社 | Polishing liquid for CMP, storage liquid for polishing liquid for CMP, and polishing method |
| JP6057706B2 (en) * | 2012-12-28 | 2017-01-11 | 株式会社フジミインコーポレーテッド | Polishing composition |
| JP2015189898A (en) * | 2014-03-28 | 2015-11-02 | 株式会社フジミインコーポレーテッド | polishing composition |
| JP2018092960A (en) * | 2015-04-03 | 2018-06-14 | Jsr株式会社 | Cleaning composition and cleaning method |
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| TWI743989B (en) * | 2019-11-15 | 2021-10-21 | 日商Ｊｓｒ股份有限公司 | Composition for chemical mechanical polishing and chemical mechanical polishing method |
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| TWI745421B (en) | 2021-11-11 |
| JP2018107294A (en) | 2018-07-05 |
| JP6819280B2 (en) | 2021-01-27 |
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